今日药学

2014, v.24(08) 556-559+563

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LC-MS/MS法测定精神分裂症合并2型糖尿病患者血浆中沙格列汀的浓度
Determination of Saxagliptin in Plasma of Schizophrenia Patients Combined with Type 2 Diabetes by LC-MS /MS

胡晋卿;张明;尚德为;倪晓佳;邱畅;王占璋;吴福喜;曾奕彬;徐昌武;文启琴;薛士健;温预关;
HU Jinqing;ZHANG Ming;SHAND Dewei;NI Xiaojia;QIU Chang;WANG Zhangzhan;WU Fuxi;ZENG Yibin;XU Changwu;WEN Qiqin;XUE Shijian;WEN Yuguan;National Drug Clinical Trial Agency,Guangzhou Hui-Ai Hospital;Department of Chronic Psychiatry,Guangzhou Hui-Ai Hospital;

摘要(Abstract):

目的建立测定精神分裂症合并2型糖尿病患者血浆中沙格列汀浓度的方法。方法血浆样品0.2 mL用醋酸乙酯-二氯甲烷(体积比4∶1)萃取,西他列汀作为内标,采用LC-MS/MS法测定。色谱柱为Agilent Eclipse plus C18(4.6 mm×150 mm,3.5μm),以甲醇-水(体积比95∶5,含0.005 mol/L甲酸铵和质量分数0.1%甲酸)为流动相,流速为0.5 mL/min,柱温为40℃;质谱条件采用ESI离子源,检测方式为正离子电离,多重反应监测(MRM),用于定量分析的离子反应分别为m/z 316.2→180.2(沙格列汀)与m/z 408.1→235.1(西他列汀)。结果沙格列汀在0.5~100μg/L(r2=0.998)范围内线性良好,其平均回收率在79.24%以上,日内、日间精密度分别小于8.30%与12.92%(次低浓度点)。结论本试验建立的沙格列汀血药浓度的测定方法简便、快速、准确、灵敏,可用于临床研究中沙格列汀的药动学研究。
Objective To establish a LC-MS /MS method for the determination of saxagliptin in plasma samples of Chinese male schizophrenia patients complicated with type 2 diabetes( T2DM). Methods Saxagliptin was extracted from plasma by ethyl acetate-dichloromethane( 4 ∶ 1). Then saxagliptin was determined by LC-MS /MS using sitagliptin as internal standards respectively. Separation carried on a Agilent Eclipse plus C18( 150 mm ×4.6 mm,5 μm) column with a mobile phase of methanol-0. 005 mol /L ammonium formate aqueous solution with 0. 1% formic acid( 95∶ 5) at the flow rate of 0.5 mL /min. The column temperature was set at 40℃. ESI source was applied and operated in positive ion mode.Quantitative determination was performed using multiple reaction monitoring( MRM) of m /z 316. 2→180. 2 for saxagliptin and m /z 408. 1→235. 1 for sitagliptin. Results Saxagliptin exhibited good linearity in the range of 0. 5- 100 μg /L( r2=0. 998). The extraction recovery for saxagliptin was more than 79. 24%,while the intra-day and inter-day precision( RSD) were lower than 8. 30% and 12. 92%,respectively. Conclusion The method is simple,rapid,accurate,and sensitive for determination of saxagliptin in human plasma,which can be applied to the clinical pharmacokineticpharmacodynamic study of saxagliptin among schizophrenia patients complicated with T2 DM.

关键词(KeyWords): 液相色谱-串联质谱法;血药浓度;血糖;沙格列汀;药代动力学-药效动力学
LC-MS /MS;plasma concentration;blood glucose;saxagliptin;pharmacokinetics-pharmacodynamics

Abstract:

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基金项目(Foundation): 广东省药学会医院药学研究基金(编号:2012C01)

作者(Author): 胡晋卿;张明;尚德为;倪晓佳;邱畅;王占璋;吴福喜;曾奕彬;徐昌武;文启琴;薛士健;温预关;
HU Jinqing;ZHANG Ming;SHAND Dewei;NI Xiaojia;QIU Chang;WANG Zhangzhan;WU Fuxi;ZENG Yibin;XU Changwu;WEN Qiqin;XUE Shijian;WEN Yuguan;National Drug Clinical Trial Agency,Guangzhou Hui-Ai Hospital;Department of Chronic Psychiatry,Guangzhou Hui-Ai Hospital;

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